- Method for preparing high-purity kerley Bette
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The invention relates to a preparation method of high-purity clinofibrate, the field of preparation of pharmaceutical compounds. The preparation method comprises the following steps: reacting cyclohexanone and phenol in concentrated hydrochloric acid and glacial acetic acid in a volume ratio of 3:1-7:1 to obtain an intermediate I crude product, decolorizing with a single solvent, and cooling to crystallize to obtain an intermediate I; reacting 2-methylbutyric acid with liquid bromine in phosphorus trichloride, reacting with anhydrous alcohol, extracting, and carrying out vacuum distillation to obtain an intermediate II; reacting the intermediate I and the intermediate II under solventless conditions to obtain an intermediate III; and hydrolyzing the intermediate III and sodium hydroxide, extracting, crystallizing to obtain a clinofibrate crude product; and recrystallizing with an anhydrous solvent to obtain the clinofibrate. The material proportion is adjusted to shorten the production operation period; the invention has the advantages of low energy consumption and low solvent consumption; and the obtained product has the advantages of uniform crystal grains, high purity and low cost.
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- Labelling of a new hypolipaemic agent with carbon 14, preparation of 1,1 bis[4 (1 carboxy 1 methylpropoxy)phenyl]cyclohexane 2 14C
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1,1 Bis[4 (1 carboxy 1 methylpropoxy)phenyl] cyclohexane (S 8527) (I), a new hypolipemic agent, was labelled as C 2 with carbon 14 for the use of metabolic studies. Cyclohexane 2 14C which was prepared from potassium cyanide 14C was condensed with phenol to produce 1,1 bis(4 hydroxyphenyl)cyclohexane 2 14C (VI). Condensation of VI with ethyl methyl ketone and chloroform under a strong base (potassium hydroxide) gave S 8527 2 14C (I). A total of 3.11 mCi of pure S 8527 2 14C (I) was obtained, representing a 12% radiochemical yield from potassium cyanide 14C. Furthermore, a new radioactive by product was isolated and elucidated its structure as X.
- Yoshitake,Makari,Kawahara,Doi
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p. 247 - 257
(2007/10/05)
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